反应详情

4′-Thiocyano-p-toluenesulfonanilide (19.2 g (63.2 mmol)) was dissolved in acetic acid (60 ml). To this, fuming nitric acid (3.04 ml (75.9 mmol)) was added dropwise with stirring at room temperature. Then, the mixture was stirred at 50° C. for 4 hours, poured into water, and the crystals separated were filtered and washed with water. The resulting crystals were dissolved in ethyl acetate, and the solution was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to give 21.8 g (99%) of 2′-nitro-4′-thiocyano-p-toluenesulfonanilide as pale yellow crystals.

1. stirringThen, the mixture was stirred at 50° C. for 4 hours
2. customthe crystals separated
3. filtrationwere filtered
4. washwashed with water
5. dissolutionThe resulting crystals were dissolved in ethyl acetate
6. dry with materialthe solution was dried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure